참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,4-Dichloro-7-methylthieno(3,2-d)pyrimidine | HCID 7147064 | — |
| 반응물 | 3-Aminopropanamide hydrochloride | HCID 22222288 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Chloro-4-(2-carbamoylethylamino)-7-methylthieno[3,2-d]pyrimidine | HCID 18326411 | 79.8% |
반응 단계
In 10 ml of DMF, 1.0 g (4.9 mmol) of 2,4-dichloro-7-methylthieno[3,2-d]pyrimidine was dissolved, and then 668 mg (5.37 mmol) of β-alanineamide hydrochloride and 1.09 g (10.7 mmol) of triethylamine were added thereto under ice cooling. The reaction solution was stirred at 0° C. for one hour and then allowed to resume room temperature, followed by stirring for further 1 hour. After completion of the reaction, ice water was added to the reaction mixture, followed by extraction with ethyl acetate (50 ml×3). After the organic layer was washed successively with 1N hydrochloric acid, water and brine and dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/8) to give 1.05 g (yield: 79.8%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06339089B2 |
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| 출처 데이터셋 | uspto-grants-2002_01 |
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| ORD ID | ord-064543062e254504b9e2a0586f065070 |
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| 출처 메모 | uspto-grants-2002_01 |
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